Search Documents

By John M. Gomes

The Bureau of Mines investigated two techniques for removing CaO from scheelite (CaW04) prior to electrolysis. In the first technique, a crude tungstic oxide (WO3) containing 0.15-percent lime (CaO) was prepared by digesting scheelite concentrates in hot hydrochloric acid. This oxide was used as cell feed to produce tungsten of 99.9-percent purity. The second technique used a high-temperature, two-phase separation, resulting in extraction of 99 percent of the WO3 in the halide-tungstate phase, while 90 percent of the CaO was retained in the silicate phase. Tungsten of 99.9-percent purity was deposited from the halide-tungstate melt after B203 and NaPO3 were added to form an electrolyte. The two methods were compared with a previously developed technique of depositing tungsten from scheelite concentrate fed directly to the electrolytic cell.

Jan 1, 1971

By L. B. Pankratz

Low-temperature heat capacities, high-temperature enthalpy increments, and the enthalpy of formation at 298° K were determined calorimetrically for vanadium subnitride (VN0.465). The low-temperature investigation gave S°298.15 = 6.379 ±0.005 cal/deg mole, and a combustion calorimeter investiga¬tion provided ?Hf°298.15 = -31.80 ±0.60 kcal/mole. The two quantities were combined with the high-temperature data to give standard values of enthalpies of formation and free energies of formation above 298° K. These and related thermodynamic functions were tabulated to 1,800° K. Similar data are included in the range of 298° to 1,600° K for the mononitride, VN.

Jan 1, 1971

By Larman J. Heath

Liquid incendiaries were burned within the interstices of several different types of sandstone cores to determine the technical feasibility of increasing sandstone permeability by this method. Fuel-oxidant mixtures were tested in 186 cores; six cores exploded when ignited. In virtually all instances, the explosion completely pulverized the sandstone cores. In addition n those cores damaged by explosions, 24 cores were fractured so severely that permeability tests were impossible. Although combustion gener¬ally increased the permeability, specific mixtures at given pressures were inconsistent in their ignition and burning behavior. Tests indicated that the heat of burning incendiaries significantly increased sandstone permeability. The improved permeability ratios were usually less than 2, but one was 10.3. Permeability alteration by other in situ methods was not as effective as that by flame propagation.

Jan 1, 1971

The Bureau of Mines has long been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts, the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions1 issued by the Bureau of Mines, and the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. The Government, with the exception of the Tennessee Valley Authority, purchased approximately 5.5 million tons of coal in fiscal year 1971. In connection with these purchases, the Bureau analyzed 4,366 samples. These are published (table 1) for the use of Government officials and the public. Such analyses of delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1972

By Thomas E. Green

A gas volumetric method was developed for determining metallic aluminum at the 0.01-to 0.3-percent level in 100-gram samples of recycled glass. The method is based on the measurement of the change in gas volume produced by the reaction 2 Al + 2 NaOH + 2 H2O ? 2 NaAl02 + 3 H2 using a simple apparatus assembled from readily available glassware. Apart from sampling errors, the precision of the method is within ±5 percent. A minor modification of the apparatus would extend the method to larger samples or samples of higher metallic aluminum content. Metallic iron and metallic zinc do not interfere at the concentrations found in recycled glass recovered from incinerator residues.

Jan 1, 1971

By M. J. Ferrante

Enthalpy and entropy increments above 298.15° K were determined for cop-per sulfate between 298° and 1,000° K and for copper oxysulfate between 2980 and 1,146° K by the method of copper-block drop calorimetry. Enthalpies, entropies, and heat capacities are tabulated for both compounds. In addition, free-energy functions are tabulated for the sulfate. Equations representing the enthalpies are given for each compound.

Jan 1, 1972

By N. N. Moebs

The atmosphere in part of an air-sealed coal mine was monitored continuously through a drill hole for oxygen content to determine the effectiveness of sealing a mine against the entrance of air and the major force that caused the phenomenon of mine breathing through the overburden. The differential pressure across the seal and the barometric pressure on the outside also were recorded. A general correlation, obtained between the oxygen level, differential pressure, and barometric pressure, indicates that changes in air pressure are the cause for periodic replenishment of the oxygen in the mine. Mine effluent quality was determined by conditions in many sections of the mine and could not be related to the oxygen level at the drill hole.

Jan 1, 1972

By G. L. Fitzpatrick

Preliminary results of an experiment in seismic holography indicate that the techniques of acoustical holography may be successfully used with seismic waves to determine the size and general shape of underground objects. This experiment was carried out under field conditions on a moderately large scale compared with the typical laboratory experiments in acoustical holography. The object to be mapped was a 100-foot-diameter, spherical, low-velocity zone of explosively fractured rock in oil shale at an average depth of 80 feet. The seismic wavelength of the Fourier component wave used in making the seismic holograms was 50 feet at a frequency of 140 cps. The hologram sampling aperture was 226 feet square and was sampled by 441 geophones in a 21 by 21 rectangular array. One novel aspect of the experiment was the use of a wide-band polychromatic explosive source of seismic waves rather than a narrow-band quasi-monochromatic vibrator source. A successful laser reconstruction of the object image from a lensless Fourier-transform hologram in the form of a 5/l6-inch-square photographic transparency is illustrated. The size of the underground object measured from the laser reconstruction of the object and the size inferred from a knowledge of the amount of explosives used to fracture the site and the tensile strength of the oil shale are found to agree.

Jan 1, 1972

By A. W. Deurbrouck

This report describes the washability characteristics of 18 coal samples taken from 11 drill hole cores from the San Juan Basin area of New Mexico and Colorado. The ash content of these coals could generally be substantially reduced by removing the heavy impurities. The coals were characteristically low in sulfur content; only one sample contained more than 1 percent sulfur after removing the sink-I.50 specific gravity material. The coals ranged in rank from subbituminous C to high volatile C; 11 of the samples were subbituminous A. Many of these core samples came from areas where very little fieldwork has been done; consequently, an outgrowth of this work has been an increase in known coal reserves of the San Juan Basin area.

Jan 1, 1972

By Joseph L. Condon

High-speed movies were taken of crater experiments in two-dimensional plates of Tennessee marble to study craters being formed primarily by stress-wave action. The contribution of gas action to the cratering process was minimized because the two-dimensional models did not contain the expanding gases from the explosive. Four burdens were studied for solid plates and one burden for a segmented plate. After cratering, the plates were reassembled for dye penetrant studies of fracturing. Flyrock velocities were calculated and related to the degree of fracturing, and compared with those from quarry shots. In general, the smallest burdens produced the highest flyrock velocities and the least amount of fracturing. Flyrock velocities compared favorably with initial flyrock velocities in quarry blasts, but did not show step accelerations due to gas effects as did the quarry blasts. The test with a segmented plate was used to simulate cratering in a jointed material and showed that stress-wave effects can be important for crater formation in jointed rocks.

Jan 1, 1972

By R. E. Peterson

Scrap iron is partially oxidized at elevated temperatures in the selective oxidation process to produce iron oxide and a dense residual metal of high purity. Investigation of the process was confined to converting automobile hulks into useful products. In one test series, compressed, sheared automobile scrap was processed at 1,000° C in a 36-foot-long rotary kiln at feed rates ranging from 300 to 1,200 lb/hr. Less fuel was required to maintain the temperature at the higher feed rates because of the heat generated from the burning of the combustibles and the oxidation of the iron. The bulk density of the residual metal exceeded 75 pounds per cubic foot. In an attempt to lower the quantity of contaminants in the residual metal, another test was designed using automobile hulks which had been prepared by ripping, a low-cost method of scrap fragmentation. Before oxidizing the ripped scrap approximately 62 percent of the total copper was removed in a tumbling, screening, magnetic separation and hand-sorting system. Cast iron made from the residual metal obtained by selective oxidation contained 0.15 percent copper; iron oxide scale obtained from the kiln averaged 0.13 percent copper. Pellets made from the scale demonstrated compressive strengths necessary for blast furnace reduction; lead and zinc were removed by volatilization when the induration was performed in a reducing atmosphere.

Jan 1, 1972

By J. A. Lamonica

The Bureau of Mines studied two types of approved coal mine dust personal samplers to determine the effect of decreasing the amplitude of airflow velocity fluctuations on cyclone performance. Results indicate that more dust is collected when pulsation free flow is used. Velocity fluctuations were reduced by means of a pulsation damper; damper efficiency of about 85 percent was needed to reduce the fluctuations to an acceptable level. The data were obtained employing both pulsating and non-pulsating flow. A comparison was made of (1) the masses of respirable coal dust as determined by weighing and of (2) the particle size distributions as determined by an electronic counter. An empirical relationship is given between the ratio of masses collected using pulsating and nonpulsating flow (M') and the ratio of the maximum air velocity to the minimum air velocity (V') as measured in the cyclone entrance channel.

Jan 1, 1972

By H. E. Powell

The smelting of brass and bronze generates a dust composed primarily of zinc oxide, with lesser amounts of other metal oxides, such as copper, lead, and tin. The small quantity of this waste generated by individual smelters and the relatively low unit value of the contained metals, suggests the desirability of reclaiming the metals onsite or at some nearby point. The Bureau of Mines has developed a process that fits these requirements. The technique consists of (1) dissolving zinc and copper from the dust with sulfuric acid, (2) recovery of copper by cementation, (3) recovery of zinc as zinc sulfate crystals, and (4) recovery of lead and tin as a salable residue. Alternatively, zinc may be recovered by electrodeposition. Free acid is recycled and no major pollution problems are generated by the process.

Jan 1, 1972

By J. M. Singer

The objective of this investigation was to determine minimum air velocities and entrainment rates for coal and rock dust dispersion in wind tunnel experiments under conditions that simulate dispersion from surfaces in coal mines where airflows are induced by weak gas explosions. Dust deposits were bed-or ridge-shaped; particle sizes were 6 to 80 microns (cohesive deposits) or 100 to 150 microns (free-flowing deposits); and wind tunnels were 7.62 cm wide by 5.08 cm high by 300 cm long, and 2.4 m wide by 1.5 m high by 215 m long. The investigation showed that minimum air velocities (directed at mid-height) of separate, layered, or mixed piles of coal dust and rock dust were within the range 5 to 30 m/sec, independent of size of wind tunnel. This finding considerably facilitates scaling of data to mine-size passageways. Free-flowing deposits dispersed relatively slowly by single-particle detachment; cohesive dusts dispersed faster by the breaking and lifting of large clumps along weak failure flames; particle dispersion occurred in flight. Layered or mixed deposits of coal and rock dust did not disperse selectively. Semiempirical expressions were derived relating minimum air velocities and dispersion rates to dust-pile geometry, cohesion, porosity, and bulk density.

Jan 1, 1972

By James L. Konchesky

Crushed coal, consisting of a wide range of sizes, was effectively blended by recycling it through a bin equipped with a particle distributor. Vertical blending was accomplished by simply recycling the coal; it was not significantly influenced by the horizontal blending that was achieved by the distributor. The method was effective, even though the coal was wet and possessed poor flowing characteristics. Recirculation appears capable of providing uniform blends of solids that can be more efficiently processed. Recirculation also appears useful, preceding packaging operations, to insure for blending of solids into specification products. Continuous measurement of the bulk density of the coal by a gamma ray meter proved to be an effective monitor of vertical blending effectiveness.

Jan 1, 1972

By M. G. Zabetakis, T. D. Moore

The use of a partially slotted 6.5-inch-inside-diameter vertical pipe to remove methane from a longwall gob area at a depth of 2,260 feet in the Pocahontas No. 3 coalbed ms investigated. The value of gas removed by such a pipe under free-flow conditions was found to equal the cost of the installation in this case. Approximately 25 percent of the available methane passed through the pipe without the use of an exhauster; an additional 10 percent was removed when an exhauster was employed. The diversion of methane through a vertical slotted pipe to the surface permitted the use of increased mining rates and decreased the ventilation air requirements.

Jan 1, 1972

By T. D. Moore

The use of a partially slotted 6.5-inch-inside-diameter vertical pipe to remove methane from a longwall gob area at a depth of 2,260 feet in the Pocahontas No. 3 coalbed was investigated. The value of gas removed by such a pipe under free-flow conditions was found to equal the cost of the installation in this case. Approximately 25 percent of the available methane passed through the pipe without the use of an exhauster; an additional 10 percent was removed when an exhauster was employed. The diversion of methane through a vertical slotted pipe to the surface permitted the use of increased mining rates and decreased the ventilation air requirements.

Jan 1, 1972

By H. E. Powell

A solvent extraction procedure was developed on a laboratory scale for recovering trisodium phosphate, zinc, and iron from waste phosphate sludge as separate products. The sludge was dissolved in hydrochloric acid, and iron was extracted as ferric chloride by isopropyl ether. Zinc was extracted by di-2-ethylhexyl phosphoric acid in kerosine. The efficiencies of the one-and two-stage extractions ranged from 98 to nearly 100 percent. Trisodium phosphate was recovered by crystallization from the raffinate. The value of two marketable products is considerably more than than the costs of the major reagent. The process was developed to permit recycling of values in this waste and to consequently reduce stream pollution from this source.

Jan 1, 1972

By R. O. Dannenberg

The Bureau of Mines investigations described in this report were undertaken to devise a process to economically recover precious metals and copper from low-grade, complex electronic scrap generated in large quantities by military and civilian electronic operations. Leaching with various media is applicable to certain selected items of electronic scrap but cannot be practically applied to complex mixtures of scrap. A process comprising incineration, caustic leaching to remove aluminum, smelting with a siliceous slag, and electrolysis recovered 99.9-percent-pure copper metal and anode slimes assaying more than 7,000 ounces per ton of combined precious metals. Silver, gold, and copper recoveries were 93, 95, and 87 percent, respectively. Cost analysis indicated that an alternative process using direct smelting of the scrap to make assayable products for sale to a custom smelter would provide better overall financial returns.

Jan 1, 1972

By Mark I. Copeland

The formation of A1203 dispersoids 0,14 and less in size in dilute iron-aluminum alloys by internal oxidation in wet hydrogen and dispersion strengthening of iron by application of the technique to iron powder were found to be feasible by the Bureau of Mines. In flowing H2-1.5 H20 gas, A1203 dispersoids 0.1w and less in size formed (at 650° to 750° C) in Fe-l and 2 Al sheet material but not in Fe-3 or 4 Al alloys. With higher temperatures and/or higher H2O/H2 volume-ratio gases, A1203 and FeA1204 dispersoids >0.14 in size formed in all the sheet materials- Minus 100-mesh Fe 2 Al powders were internally oxidized under conditions that promoted formation of fine A1203 particles in sheet material, and then the oxidized powders were hydrogen reduced, sintered, extruded, and evaluated. During internal oxidation, fine A1203 dispersoids formed within the powder grains, and coarse FeA1204 particles formed on the powder surfaces and grain boundaries. The FeA1204 content was essentially eliminated during sintering by reacting with the unoxidized aluminum that remained in the center of the larger internally oxidized powders. The tensile strength at 800° C depended upon the aluminum-oxygen weight ratio of these elements in the extrusions and reached a maximum of 17,000 psi. The stress-rupture strengths at 800° C of the better alloys were comparable with those of type 310 stainless steel.

Jan 1, 1972